Phosphorus oxychloride → HCID 178506089, 화합물

HRID 496256

반응식

HRID 496256 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:12]=[CH:11][C:6]2[NH:7][C:8](=O)[NH:9][C:5]=2[CH:4]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:8]1[NH:7][C:6]2[CH:11]=[CH:12][C:3]([C:2]([F:14])([F:13])[F:1])=[CH:4][C:5]=2[N:9]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 118201505-Trifluoromethyl-1,3-dihydro-benzimidazol-2-one

생성물 1

HCID 178506089HCID 178506089, 화합물

실험 절차

Reflux 5-trifluoromethyl-1,3-dihydro-benzimidazol-2-one (17 g; Meanwell et al. (1995) J. Org. Chem. 60(6):1565-1582) for 14 hours in POCl3 (200 mL). Evaporate the solvent in vacuo, then carefully neutralize with saturated NaHCO3, and extract with EtOAc. Dry over Na2SO4, concentrate under vacuum, and purify by flash chromatography (1:1 hexanes/EtOAc) to obtain 2-chloro-5-trifluoromethyl-1H-benzimidazole. B. 1′-(5-Trifluoromethyl-1H-benzimidazol-2-yl)-spiro[isobenzofuran-1,4′-piperidin]-3-one hydrochloride

후처리

  1. customEvaporate the solvent in vacuo
  2. extractionextract with EtOAc
  3. dry with materialDry over Na2SO4
  4. concentrationconcentrate under vacuum
  5. custompurify by flash chromatography (1:1 hexanes/EtOAc)

출처 및 근거

ORD 기록
ord-71967602e6af4430b1cc7bd91ac17548
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943199B2

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